WO2000005573A1 - Detecteur de gaz et son procede de fabrication - Google Patents

Detecteur de gaz et son procede de fabrication Download PDF

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Publication number
WO2000005573A1
WO2000005573A1 PCT/DE1999/001727 DE9901727W WO0005573A1 WO 2000005573 A1 WO2000005573 A1 WO 2000005573A1 DE 9901727 W DE9901727 W DE 9901727W WO 0005573 A1 WO0005573 A1 WO 0005573A1
Authority
WO
WIPO (PCT)
Prior art keywords
layer
gas sensor
base
base layer
measuring electrode
Prior art date
Application number
PCT/DE1999/001727
Other languages
German (de)
English (en)
Inventor
Jens Stefan Schneider
Harald Neumann
Johann Riegel
Frank Stanglmeier
Bernd Schumann
Original Assignee
Robert Bosch Gmbh
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Robert Bosch Gmbh filed Critical Robert Bosch Gmbh
Priority to EP99938187A priority Critical patent/EP1040346B1/fr
Priority to DE59914732T priority patent/DE59914732D1/de
Priority to JP2000561489A priority patent/JP2002521662A/ja
Priority to US09/509,270 priority patent/US6395161B1/en
Publication of WO2000005573A1 publication Critical patent/WO2000005573A1/fr

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/406—Cells and probes with solid electrolytes
    • G01N27/407—Cells and probes with solid electrolytes for investigating or analysing gases
    • G01N27/4075—Composition or fabrication of the electrodes and coatings thereon, e.g. catalysts
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/406—Cells and probes with solid electrolytes
    • G01N27/407—Cells and probes with solid electrolytes for investigating or analysing gases
    • G01N27/4071—Cells and probes with solid electrolytes for investigating or analysing gases using sensor elements of laminated structure
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/406—Cells and probes with solid electrolytes
    • G01N27/407—Cells and probes with solid electrolytes for investigating or analysing gases
    • G01N27/4077—Means for protecting the electrolyte or the electrodes

Definitions

  • the invention relates to a gas sensor according to the preamble of claim 1 and to a method for producing the gas sensor.
  • a sensor is known in which an electrode made of gold or silver which does not catalyze the equilibrium of the gas mixture is provided and which interacts with an electrode made of platinum which catalyzes the equilibrium of the measurement gas.
  • the catalytically inactive electrode materials cause a competitive reaction to take place on the electrode between the oxygen and the oxidizable or reducible gas components.
  • the free oxygen carried in the sample gas is hardly converted with, for example, C3H 5 or CO, so that both free oxygen and C3Hg or CO reach the three-phase limit at the catalytically inactive electrode (un- state of equilibrium).
  • the measuring electrode consists of a platinum compound or a ternary alloy of platinum, gold, nickel, copper, rhodium, ruthenium, palladium or titanium.
  • the materials can also be applied as multiple layers on the solid electrolyte, the alloying step taking place after the materials have been applied.
  • a gas sensor is also known from US Pat. No. 4,199,425, in which a platinum electrode is provided which is covered with a porous cover layer.
  • Another catalytic material, rhodium is introduced into the pores of the cover layer by impregnation.
  • the rhodium has the task of making the gas sensor sensitive to NO x in addition to its sensitivity to oxygen.
  • the rhodium lies in the walls of the pores of the entire cover layer, so that no specific layer thickness can be formed in the porous cover layer.
  • the gas sensor according to the invention with the characterizing features of claim 1 has the advantage that a sintered sensor element base body can be used, only the further layer after sintering being integrated by an additional deposition step.
  • the outer electrode of the sensor element base body can be modified after sintering.
  • the sensor element of a lambda probe of the Nernst type for example, can be used as the sensor element base body, the modification of the outer electrode transforming it into a mixed potential electrode. It is also advantageous that materials can be used for the further layers that would otherwise not withstand the high sintering temperature.
  • Another advantage is that the immediately Another layer system arranged adjacent to the electrically conductive base layer does not completely fill the pores of the porous cover layer.
  • the material of the additional layer is used to specifically modify the functional properties of the electrode of the gas sensor.
  • the modification can serve to set the specific gas selectivity and / or the control position of the sensor.
  • Layer the layer system is subjected to a thermal aftertreatment.
  • a temperature range of 1200 ° C ⁇ 100 ° C has proven to be favorable for a Pt / Au electrode.
  • the metal atoms of the further layer diffuse into the metal of the neighboring base layer.
  • a cermet layer is used as the electrically conductive base layer, which due to its ceramic component forms a firm connection with the solid electrolyte during sintering of the ceramic body.
  • the formation of several further layers and a suitable choice of material for the layers also make it possible to modify the catalytic activity of the electrode in a more targeted manner in addition to setting the selectivity.
  • FIG. 1 shows a section through an invented gas sensor according to the invention
  • Figure 2 is an enlarged sectional view of a first embodiment of an electrode of the gas sensor of the invention
  • Figure 3 is an enlarged sectional view of a second embodiment of an electrode of the gas sensor of the invention.
  • FIG. 1 shows a gas sensor with a sensor element base body 10, which has a structure of the kind used for oxygen sensors of the Nernst type (lambda probes).
  • the base body 10 is constructed, for example, from a plurality of ceramic solid electrolyte foils 11, 12, 13, which consist, for example, of ZrO 2 stabilized with Y 2 O 3 .
  • An outer measuring electrode 15 with an overlying porous cover layer 16 is arranged on the outer large surface of the first film 11.
  • the cover layer 16 consists, for example, of porous ZrÜ 2 or Al 2 O 3 .
  • a reference channel 17 is introduced into the second film 12 and is connected to a reference atmosphere, for example air.
  • a heating device 22 is also integrated in the base body 10, electrical insulation layers 21 in which the heating device 22 is embedded being applied to the third film 13. The heater 22 is operated as an electrical resistance heater.
  • the measuring electrode 15 has the layer structure shown in FIG. 2. Then there is an electrically conductive base layer 25 made of, for example, a Pt cermet on the film 11 of the base body 10.
  • the cover layer 16 lies on the base layer 25. According to FIG. 2, the cover layer 16 is adjacent in the pores a further layer 27 is formed on the base layer 25. This layer 27 is in direct contact with the base layer 25.
  • the base layer 25 and the further layer 27 form the measuring electrode 15. The production of the layer 27 will be discussed later.
  • the layer 27 can consist of a material that inhibits or inhibits the equilibrium of the gas mixture on the electrode surface.
  • materials are, for example, noble metals (gold, rhodium, iridium), semi-precious metals (palladium, silver), base metals (copper, bismuth, nickel, chromium) or a mixture of these metals.
  • the further layer 27 consists of gold.
  • Mixed potential electrodes are electrodes that cannot or only partially catalyze the equilibrium of the gas mixture.
  • the measuring electrode 15 forms, together with the reference electrode 18 arranged in the reference channel 17 from Pt, for example, a so-called mixed potential sensor.
  • the material of the layer 27 of the measuring electrode 15 which does not or does not completely catalyze the equilibrium of the gas mixture has the effect that a competitive reaction takes place at the measuring electrode 15 between the oxygen and the oxidizable gas components. Accordingly, the CO carried in the sample gas is hardly converted to CO 2 with the free oxygen. As a result, both free oxygen and CO reach the three-phase
  • Limit of the measuring electrode 15 and contributes to the signal formation there.
  • a potential difference is formed between the measuring electrode 15 and the reference electrode 18, at which a constant oxygen partial pressure is present with the reference air, and is measured as an EMF by a measuring instrument 30. that can.
  • the EMF is therefore dependent on the oxidizable gas components.
  • the selectivity of the measuring electrode 15 can thus be specifically adjusted to a gas species by a corresponding choice of material for the further layer 27, so that the cross-sensitivity to other gas components is reduced.
  • the low temperature behavior of an oxygen sensor can be improved by a Rh layer on a Pt electrode.
  • FIG. 3 A second exemplary embodiment of a layer system for the measuring electrode 15 is shown in FIG. 3.
  • the layer 27 is formed above the base layer 25 in the pores of the cover layer 16 and a second layer 28 is formed above the layer 27 and a third layer 29 is formed above the layer 28.
  • layer 27 consists for example of gold, layer 28 for example of rhodium or iridium and layer 29 of nickel or chromium.
  • layer 29 of nickel or chromium.
  • This example shows that a complicated, multilayered electrode structure can be realized in a simple manner.
  • the layer structure shown in FIG. 3 and / or by an appropriate choice of material for the layers 27, 28, 29, z. B. specifically modify the catalytic properties of the electrode.
  • the sensor element base body 10 described is used to manufacture the sensor according to FIG.
  • the foils 11, 12, 13 are provided with the corresponding functional layers in the green (unsintered) state.
  • the first film 11 is printed on one large area with a Pt cermet paste for producing the base layer 25 and on the other large area also with a Pt cermet paste for producing the reference electrode 18.
  • the top layer 16 is applied to the large area of the film 11 via the Pt-cermet paste of the base layer 25 by, for example, screen printing or brushing.
  • the Material of the cover layer 16 contains pore formers which evaporate or burn during later sintering and thereby form the pores.
  • the insulation layers 21 and the heating device 22 between the insulation layers 21 are printed on the film 13 in screen printing steps.
  • the films 11 and 13 printed in this way with the functional layers are laminated together with the film 12, into which the reference channel 17 was previously punched, and sintered at a temperature of, for example, 1400 ° C.
  • the base body 10 After sintering, the base body 10 is present, which corresponds to the construction of a sensor element of an oxygen sensor for determining the lambda value in gas mixtures.
  • the base body 10 present in the sintered state is provided with a layer 27 according to FIG. 2 or with a plurality of layers 27, 28, 29 according to FIG. 3, the layer 27 or the layers 27, 28, 29 in the layer planes in the Pores of the porous cover layer 16 are formed.
  • the layers 27, 28, 29 are produced by electrodeposition.
  • the ceramic body is placed in a galvanic bath.
  • the base layer 25 is electrically connected as a cathode, the connection contact of the base layer present on the sensor element base body 10
  • the anode for example, a metal is immersed in the electroplating bath, which corresponds to the metal of the layer 27, 28, 29 to be deposited in each case (galvanic process with sacrificial anode).
  • the electrolytes used are, for example, water-soluble, ionic salts of the metals in question, such as, for example, HAuCl 4 , IrCl3 x H2O or RI1CI3 x H 2 0.
  • a layer system according to FIG. 2 is selected for the production of a sensor for the determination of hydrocarbons.
  • a gold layer is electrodeposited on the base layer 25 made of Pt cermet.
  • the sintered base body 10 is placed in an electroplating bath with a HAUCI4 electrolyte, a gold anode being used.
  • the layer 27 made of gold is deposited on the Pt-Cermet base layer 25 with a layer thickness of, for example, 1-5 ⁇ m.
  • the layer 27 forms in the pores of the cover layer 16.
  • the ceramic body is subjected to an annealing treatment at a temperature of, for example, 1200 ° C.
  • an alloy is formed between the Pt of the base layer 25 and the gold of the layer 27, namely a platinum-rich gold phase and a gold-rich platinum phase.
  • the catalytic activity of the Pt of the Pt-cermet base layer 25 is modified and a mixed potential electrode is formed as the measuring electrode 15, which is selective towards hydrocarbons.
  • the layer system according to FIG. 3 is likewise produced by electroplating, the corresponding anode materials and / or the corresponding electroplating baths being used in succession in the electroplating.
  • the corresponding anode materials and / or the corresponding electroplating baths being used in succession in the electroplating.
  • Layer systems further combinations and layer systems for electrodes of gas sensors are also conceivable, which are deposited in a porous layer on an electrically conductive base layer.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Molecular Biology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Measuring Oxygen Concentration In Cells (AREA)

Abstract

L'invention concerne un détecteur de gaz ainsi que son procédé de fabrication. Ce détecteur de gaz présente un électrolyte solide (11) possédant au moins une électrode de mesure (15) et une couche de revêtement poreuse (16). L'électrode de mesure (15) est réalisée avec une couche de base (25) électroconductrice et une autre couche (27), cette autre couche (27) formée au voisinage de la couche de base (25) dans les pores de la couche de revêtement poreuse (16) étant séparée par voie galvanique. Pour la séparation galvanique de l'autre couche (27), un corps de base (10) fritté avec la couche de base (25) et la couche de revêtement (16) est plongé dans un bain de galvanisation, et la couche de base (25) est mise en circuit comme cathode.
PCT/DE1999/001727 1998-07-23 1999-06-12 Detecteur de gaz et son procede de fabrication WO2000005573A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP99938187A EP1040346B1 (fr) 1998-07-23 1999-06-12 Detecteur de gaz a electrolyte solide et son procede de fabrication
DE59914732T DE59914732D1 (de) 1998-07-23 1999-06-12 Festelektrolyt-gassensor und verfahren zu dessen herstellung
JP2000561489A JP2002521662A (ja) 1998-07-23 1999-06-12 ガスセンサおよびその製造方法
US09/509,270 US6395161B1 (en) 1998-07-23 1999-06-12 Gas sensor and corresponding production method

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19833087A DE19833087A1 (de) 1998-07-23 1998-07-23 Gassensor und Verfahren zu dessen Herstellung
DE19833087.1 1998-07-23

Publications (1)

Publication Number Publication Date
WO2000005573A1 true WO2000005573A1 (fr) 2000-02-03

Family

ID=7874996

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE1999/001727 WO2000005573A1 (fr) 1998-07-23 1999-06-12 Detecteur de gaz et son procede de fabrication

Country Status (5)

Country Link
US (1) US6395161B1 (fr)
EP (1) EP1040346B1 (fr)
JP (1) JP2002521662A (fr)
DE (2) DE19833087A1 (fr)
WO (1) WO2000005573A1 (fr)

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EP1213581A2 (fr) * 2000-11-20 2002-06-12 Delphi Technologies, Inc. Détecteur de gaz avec électrode de référence sélective et son procédé de fabrication
EP1213582A3 (fr) * 2000-12-07 2003-12-17 Denso Corporation Elément capteur de gaz

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EP0372425A2 (fr) * 1988-12-02 1990-06-13 Ngk Spark Plug Co., Ltd Elément de détection d'oxygène et sa méthode de fabrication
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DE4100106C1 (fr) * 1991-01-04 1992-05-27 Robert Bosch Gmbh, 7000 Stuttgart, De
DE4131503A1 (de) * 1991-09-21 1993-04-01 Bosch Gmbh Robert Abgassensor und verfahren zu dessen herstellung
DE4408504A1 (de) * 1994-03-14 1995-09-21 Bosch Gmbh Robert Sensor zur Bestimmung der Konzentration von Gaskomponenten in Gasgemischen
DE19700700A1 (de) * 1997-01-13 1998-07-16 Bosch Gmbh Robert Sensorelement und Verfahren zu dessen Herstellung

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1213581A2 (fr) * 2000-11-20 2002-06-12 Delphi Technologies, Inc. Détecteur de gaz avec électrode de référence sélective et son procédé de fabrication
EP1213581A3 (fr) * 2000-11-20 2003-12-03 Delphi Technologies, Inc. Détecteur de gaz avec électrode de référence sélective et son procédé de fabrication
EP1213582A3 (fr) * 2000-12-07 2003-12-17 Denso Corporation Elément capteur de gaz
US6949175B2 (en) 2000-12-07 2005-09-27 Denso Corporation Gas sensing element

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JP2002521662A (ja) 2002-07-16
DE59914732D1 (de) 2008-05-29
EP1040346A1 (fr) 2000-10-04
EP1040346B1 (fr) 2008-04-16
US20020023838A1 (en) 2002-02-28
US6395161B1 (en) 2002-05-28
DE19833087A1 (de) 2000-01-27

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